HPLC测定川楝子不同采收期及不同部位中川楝素的含量

通过测定不同采收期和不同部位川楝子中川楝素的含量,为确定川楝子最佳采收期提供依据。采用高效液相色谱法,色谱柱Agilent Zorbax SB-C18（4.6mm×150mm,5μm）,流动相乙腈—水（28∶72）,流速1.0mL/min,检测波长210nm,柱温35℃。不同采收期川楝子中川楝素以1—2月间采收的含量最高;同一采收期的川楝子果核和果肉中川楝素含量最高,外果皮次之,种子中未检出川楝素。     

A New Approach to Plant Diversity Assessment Combining HPLC Data, Simplex Mixture Design and Discriminant Analysis

The quantitative assessment of plant diversity and its monitoring with time represent a key environmental issue for management and conservation of natural resources. Assessment of plant diversity could be based on chemical analyses of secondary metabolites (e.g. flavonoids, terpenoids), because of the substantial quantitative and qualitative between-individual variability in such compounds. At a geographical scale, the plant populations become widely dispersed, and their monitoring from numerous routine individual analyses could become restricting. To overcome such constraint, this study develops a multivariate calibration model giving the relative frequency of a particular taxon from a simple high-performance liquid chromatography (HPLC) analysis of a plant mixture. The model was built from a complete set of mixtures combining different taxons, according to an experimental design (Scheffé’s matrix). For each mixture, a reference HPLC pattern was simulated by averaging the individual HPLC profiles of the constitutive taxons. The calibration models, based on Bayesian discriminant analysis (BDA), gave statistical relationships between the contributions of each taxon in mixtures and reference HPLC patterns of these mixtures. Finally, these models were validated on new mixtures by using outside plants. This new biodiversity survey approach is illustrated on four chemical taxons (four chemotypes) of Astragalus caprinus (Fabaceae). The more differentiated the taxon, the better predicted its contributions (in mixtures) were by BDA calibration model. This new approach could be very useful for a global routine survey of plant diversity.     

不同环境介质中异丙隆残留的前处理方法研究

利用高效液相色谱法(HPLC)测定水、土壤和植物中除草剂异丙隆的残留量.采用LC-18固相萃取小柱分离、净化和富集水中异丙隆残留;利用丙酮/水(体积比为3:1)振荡提取土壤中的异丙隆残留,并通过硅胶柱层析净化、分离;以乙酸乙酯为提取剂,采用超声波提取植物样品中的异丙隆残留,并用Florisil固相萃取小柱净化、分离.利用HPLC-UVD(Ultraviolet Detector,紫外检测器)定性、定量测定水、土壤和植物样品中异丙隆残留量.结果表明,异丙隆HPLC的线性检测范围为0.1～16 mg/L,决定系数\%R2\%=0.999 9,最低检测浓度为0.012 mg/L.水的加标回收率为90.7%～91.1%,相对标准偏差为3.0%～12.0%;土壤的加标回收率为88.4%～97.4%,相对标准偏差为6.9%～9.8%;植物的加标回收率为94.4%～99.9%,相对标准偏差为4.6%～9.0%.研究为异丙隆残留的检测提供了一种有效方法.     

高效液相色谱法测定土壤中三嗪类除草剂

建立了索氏提取、中性氧化铝小柱净化、高效液相色谱二极管阵列检测器测定土壤中7种三嗪类除草剂的方法，优化了检测波长、提取方法和溶剂、梯度淋洗程序等试验条件。7种三嗪类除草剂在0．10mg／L～2．00mg／L范围内线性良好，检出限为0．84μg／kg～2．07μg／kg，RSD为1．2％～5．6％，加标回收率为95.0％～107％。     

河豚毒素检测技术研究进展

对检测河豚毒素的主要方法包括生物检测方法、理化检测方法、免疫学方法、传感器方法进行了介绍,并对目前检测方法的优缺点进行比较分析。小鼠测定法是河豚毒素检测的标准方法;理化检测法方法准确,但是对设备要求高,前处理严格;免疫学方法费用较高;传感器方法是新方法,还有待进一步规范。各种检测方法都有其优缺点,河豚毒素检测时应根据要求选择方法。     

高效液相色谱法测定水中7种三嗪类除草剂

采用液液萃取和固相萃取两种方法预处理,高效液相色谱二极管阵列检测器测定水中7种三嗪类除草剂,选择了合适的检测波长和梯度淋洗条件。方法在0.100 mg/L~2.00 mg/L范围内线性良好,检出限为0.06μg/L~0.15μg/L,水样平行测定的RSD为1.6%~6.5%,加标回收率为95.0%~106%。     

液相色谱法测定土壤中对羟基苯甲醛

采用加速溶剂萃取法萃取土壤中的对羟基苯甲醛,用HPLC进行定量分析,判断液相色谱法测定土壤中对羟基苯甲醛的方法可行性。研究表明,该方法具有分离效果较好,前处理简单、快速准确、灵敏度高、重复性好等特点,适用于土壤中对羟基苯甲醛的测定。     

Development and application of LC–APCI–MS method for biomonitoring of animal and human exposure to imidacloprid

Imidacloprid (IMI) is a relatively new neuro-active neonicotinoid insecticide and nowadays one of the largest selling insecticides worldwide. In the present study a LC–APCI–MS based method was developed and validated for the quantification of imidacloprid and its main metabolite 6-chloronicotinic acid (6-CINA) in urine and hair specimens. The method was tested in biomonitoring of intentionally exposed animals and subsequently applied for biomonitoring of Cretan urban and rural population.     

Matrine and oxymatrine in corroborant plant extracts and fertilizers: HPLC/MS-MS method development and single-laboratory validation

A reversed phase high-performance liquid chromatographic method (HPLC/MS-MS) has been developed and validated for detection of alkaloids matrine and oxymatrine in fertilizer with labeled enhancer plant defense activities. The analytical method was validated statistically. The results show a strong matrix effect, requiring quantification by standard addition method. The regression lines showed r² > 0.994. Recoveries ranging from 97 to 104% were obtained for the fortification level of 0.01% wt wt^?1 and the relative standard deviations ranged from 3 to 4% (n = 10). The limits of detection were below 0.0001% wt wt^?1, while the limits of quantification did not exceed 0.0004% wt wt^?1. The method is currently applied in ICQRF Laboratory of Catania on fertilized and corroborant plant extract collected in the Italian market in the frame of MIPAAF institutional quality control activity, with the aim to dectect these unpermitted active substances.     

Viable skin efficiently absorbs and metabolizes bisphenol A

Skin contact has been hypothesized to contribute to human exposure to bisphenol A (BPA). We examined the diffusion and metabolism of BPA using viable skin models: human skin explants and short-term cultures of pig ear skin, an alternative model for the study of the fate of xenobiotics following contact exposure. ¹⁴C-BPA [50-800 nmol] was applied on the surface of skin models. Radioactivity distribution was measured in all skin compartments and in the diffusion cells of static cells diffusion systems. BPA and metabolites were further quantified by radio-HPLC. BPA was efficiently absorbed in short-term cultures, with no major difference between the models used in the study [viable pig ear skin: 65%; viable human explants: 46%; non-viable (previously frozen) pig skin: 58%]. BPA was extensively metabolized in viable systems only. Major BPA metabolites produced by the skin were BPA mono-glucuronide and BPA mono-sulfate, accounting together for 73% and 27% of the dose, in pig and human, respectively. In conclusion, experiments with viable skin models unequivocally demonstrate that BPA is readily absorbed and metabolized by the skin. The trans-dermal route is expected to contribute substantially to BPA exposure in human, when direct contact with BPA (free monomer) occurs.